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FE Simulation of SMA Seal for Mars Sample Return

Several NASA rovers and landers have been on Mars and performed successful in-situ exploration. Returning Martian samples to Earth for extensive analysis is of great interest to the planetary science community. Current Mars sample return architecture would require leaving the acquired samples on Mars for years before being retrieved by subsequent mission. Each sample would be sealed securely to keep its integrity. A reliable seal technique that does not affect the integrity of the samples and uses a simple low-mass tool is required. The shape memory alloy (SMA) seal technique is a promising candidate. A study of the thermal performances of several primary designs of a SMA seal for sample tubes by finite element (FE) simulation are presented in this paper. The results show sealing the sample tube by SMA plugs and controlling the sample temperature below the allowed temperature level are feasible.

seal↗

Overview of the Capture, Containment, and Return System (CCRS)

The Mars Sample Return (MSR) campaign is one of the most ambitious and complex planetary exploration missions currently underway. With the participation of NASA, ESA, and a large number of industry partners, MSR aims to bring Martian soil, rock, and atmospheric samples back to Earth, in order to answer key questions about Mars’ biological evolution. To accomplish this goal the campaign relies on four coordinated missions, each fulfilling a fundamental role to bring the samples to Earth. The Mars Perseverance rover, the first of the four missions, landed safely on Mars on February 18, 2021 and has already acquired candidate samples for Earth return. A selection of the samples of Martian soil and atmosphere that Perseverance has captured during its mission will be recovered, launched into Mars orbit, and transported back to Earth. The Sample Fetch Rover and Mars Ascent System, both parts of the Sample Return Lander project, perform the Mars surface missions to retrieve the collected samples and launch them into Mars orbit. NASA’s Capture, Containment, and Return System (CCRS), hosted on ESA’s Earth Return Orbiter (ERO), brings the samples back to Earth from Mars orbit. These retrieval and return missions are currently in the planning and design stages of development. The NASA-provided CCRS is the payload of the ESA ERO and is the focus of this presentation. ERO will enter Mars orbit and provide communication relay to Earth for the other MSR elements. The Sample Return Lander systems will fetch the sample tubes and integrate them into a protective vessel – the Orbiting Sample (OS) system – which is then launched into low Mars orbit. ERO will perform rendezvous maneuvers, allowing its CCRS payload to capture the OS, contain it, and perform the first automated in-space assembly of a spacecraft, the Earth Entry System (EES), while in Mars orbit. ERO will then begin its journey back to Earth, with CCRS and its assembled EES spacecraft. Three days prior to arrival, CCRS will release the EES on an Earth entry trajectory from a distance beyond the orbit of the Moon. The passive EES spacecraft will then enter Earth’s atmosphere, flying on a ballistic trajectory, followed by a terminal descent (without a parachute) and landing at the Utah Test and Training Range (UTTR). This presentation will show the current design of the CCRS system and its concept of operations. ERO and CCRS will perform several firsts in planetary exploration: (a) orbital rendezvous and capture in Mars orbit, (b) in-space sterilization and containment, (c) on-orbit spacecraft assembly at Mars, and (d) fully-passive entry, descent, and landing sequence for sample return.

Carlie H. Zumwalt↗

Development of Cryogenic Phase Change Materials for Lunar Sample Return

One of the scientific goals of NASA’s Artemis missions is to return regolith samples from the lunar surface. To maintain scientific integrity of these samples, including any volatiles that may exist, cryogenic stowage is desired. FROSTE (Frozen Return Of Samples To Earth) is the element of the Moon to Mars architecture that is tasked with developing and advancing concepts related to this goal. Both active and passive solutions are being considered, but active solutions (cryo-coolers) have high mass and cost penalties. Phase change materials (PCMs) are commonly used as passive thermal management solutions, particularly for sensitive scientific samples. However, there are currently no PCMs capable of providing cooling at the cryogenic temperatures needed to enable lunar sample return with volatiles intact (<120 K). FROSTE has identified two possible candidate materials that could fill this gap. Testing is required to verify the thermal performance of these materials, as well as gain experience with their handling characteristics. We are conducting this testing at the Marshall Space Flight Center’s Space Environmental Effects laboratory, in vacuum, with liquid nitrogen providing cooling ability below the freezing point of the materials. In this talk, we will present an overview of the FROSTE program element and share results from the initial development testing of two cryogenic phase change materials.

phase change material↗

Harnessing quantum light for microscopic biomechanical imaging of cells and tissues

The biomechanical properties of cells and tissues play an important role in our fundamental understanding of the structures and functions of biological systems at both the cellular and subcellular levels. Recently, Brillouin microscopy, which offers a label-free spectroscopic means of assessing viscoelastic properties in vivo, has emerged as a powerful way to interrogate those properties on a microscopic level in living tissues. However, susceptibility to photodamage and photobleaching, particularly when high-intensity laser beams are used to induce Brillouin scattering, poses a significant challenge. This article introduces a transformative approach designed to mitigate photodamage in biological and biomedical studies, enabling nondestructive, label-free assessments of mechanical properties in live biological samples. By leveraging quantum-light-enhanced stimulated Brillouin scattering (SBS) imaging contrast, the signal-to-noise ratio is significantly elevated, thereby increasing sample viability and extending interrogation times without compromising the integrity of living samples. The tangible impact of this methodology is evidenced by a notable three-fold increase in sample viability observed after subjecting the samples to three hours of continuous squeezed-light illumination, surpassing the traditional coherent light-based approaches. The quantum-enhanced SBS imaging holds promise across diverse fields, such as cancer biology and neuroscience where preserving sample vitality is of paramount significance. By mitigating concerns regarding photodamage and photobleaching associated with high-intensity lasers, this technological breakthrough expands our horizons for exploring the mechanical properties of live biological systems, paving the way for an era of research and clinical applications.

Li, Tian↗

Radiant source tracker independent of nonconstant irradiance

A tracker of a radiant source is disclosed. The tracker is composed of a sectored matrix of detectors whose output voltages correspond to their respective levels of irradiance. The voltages are each sampled during a variable length period and the resulting samples are shaped into triangular samples by an integration process. They are supplied to a demodulator which provides an output corresponding to the difference of the time-voltage product of appropriate combinations of the samples. This output, after filtering, represents the angle of incidence on the detectors with respect to a central axis. The triangular samples are also supplied to a demodulator whose output is an AGC voltage which is a function of the sum of the time-voltage integrals of the triangular samples.

Campbell, F. D.↗

An Integrated Tool for System Analysis of Sample Return Vehicles

The next important step in space exploration is the return of sample materials from extraterrestrial locations to Earth for analysis. Most mission concepts that return sample material to Earth share one common element: an Earth entry vehicle. The analysis and design of entry vehicles is multidisciplinary in nature, requiring the application of mass sizing, flight mechanics, aerodynamics, aerothermodynamics, thermal analysis, structural analysis, and impact analysis tools. Integration of a multidisciplinary problem is a challenging task; the execution process and data transfer among disciplines should be automated and consistent. This paper describes an integrated analysis tool for the design and sizing of an Earth entry vehicle. The current tool includes the following disciplines: mass sizing, flight mechanics, aerodynamics, aerothermodynamics, and impact analysis tools. Python and Java languages are used for integration. Results are presented and compared with the results from previous studies.

Samareh, Jamshid A.↗

Automation of Laser Plasma Focused Ion Beam Microscopy for Next-Gen Energy Materials

Automation can revolutionize the use of ultrafast laser ablation and plasma-focused ion beam (PFIB) techniques for high-throughput, reproducible cross-sectioning and various sample preparation in materials characterization. As these methods become essential for analyzing complex energy materials and next-generation devices, efficient, standardized workflows are needed to minimize variability and enhance precision. This work highlights our advancements in developing automated processes for sample preparation that integrates machine learning, workflow optimization, and large-scale data acquisition to improve efficiency and scalability in applications such as electrolyzers, photovoltaic cells, and microelectronics. To streamline cross-sectioning and lamella fabrication, we have implemented fully automated workflows that standardize laser ablation and PFIB milling sequences. These workflows incorporate pre-programmed protocols for material removal, alignment, and thinning, reducing user intervention and ensuring consistency across different sample types. Machine learning algorithms further enhance automation by predicting optimal milling strategies and adapting parameters based on material properties and sectioning requirements. This approach significantly improves throughput while maintaining the structural integrity of prepared samples for high-resolution imaging and analysis, including transmission electron microscopy. Beyond sample preparation, our automation platform enables the acquisition of large, high-resolution datasets through serial sectioning, image alignment, and 3D reconstruction. These automated routines facilitate multi-scale characterization, capturing structural and compositional details from the nanoscale to the device level. By reducing variability and increasing efficiency, our automated approach enhances defect analysis, failure diagnostics, and process optimization, accelerating advancements in materials research and device engineering.

36 MATERIALS SCIENCE↗

Future of the Search for Life: Workshop Report

The 2-week, virtual Future of the Search for Life science and engineering workshop brought together more than 100 scientists, engineers, and technologists in March and April 2022 to provide their expert opinion on the interconnections between life-detection science and technology. Participants identified the advances in measurement and sampling technologies they believed to be necessary to perform in situ searches for life elsewhere in our Solar System, 20 years or more in the future. Among suggested measurements for these searches, those pertaining to three potential indicators of life termed “dynamic disequilibrium,” “catalysis,” and “informational polymers” were identified as particularly promising avenues for further exploration. For these three indicators, small breakout groups of participants identified measurement needs and knowledge gaps, along with corresponding constraints on sample handling (acquisition and processing) approaches for a variety of environments on Enceladus, Europa, Mars, and Titan. Despite the diversity of these environments, sample processing approaches all tend to be more complex than those that have been implemented on missions or envisioned for mission concepts to date. The approaches considered by workshop breakout groups progress from nondestructive to destructive measurement techniques, and most involve the need for fluid (especially liquid) sample processing. Sample processing needs were identified as technology gaps. These gaps include technology and associated sampling strategies that allow the preservation of the thermal, mechanical, and chemical integrity of the samples upon acquisition; and to optimize the sample information obtained by operating suites of instruments on common samples. Crucially, the interplay between science-driven life-detection strategies and their technological implementation highlights the need for an unprecedented level of payload integration and extensive collaboration between scientists and engineers, starting from concept formulation through mission deployment of life-detection instruments and sample processing systems.

Marc Neveu↗

Sample Processor for Life on Icy Worlds (SPLIce): Design and Test Results

We report the design, development, and testing of the Sample Processor for Life on Icy Worlds (SPLIce) system, a microfluidic sample processor to enable autonomous detection of signatures of life and measurements of habitability parameters in Ocean Worlds. This monolithic fluid processing-and-handling system (Figure 1; mass 0.5 kg) retrieves a 50-L-volume sample and prepares it to supply a suite of detection instruments, each with unique preparation needs. SPLIce has potential applications in orbiter missions that sample ocean plumes, such as found in Saturns icy moon Enceladus, or landed missions on the surface of icy satellites, such as Jupiters moon Europa. Answering the question Are we alone in the universe? is captivating and exceptionally challenging. Even general criteria that define life very broadly include a significant role for water [1,2]. Searches for extinct or extant life therefore prioritize locations of abundant water whether in ancient (Mars), or present (Europa and Enceladus) times. Only two previous planetary missions had onboard fluid processing: the Viking Biology Experiments [3] and Phoenixs Wet Chemistry Laboratory (WCL) [4]. SPLIce differs crucially from those systems, including its capability to process and distribute L-volume samples and the integration autonomous control of a wide range of fluidic functions, including: 1) retrieval of fluid samples from an evacuated sample chamber; 2) onboard multi-year storage of dehydrated reagents; 3) integrated pressure, pH, and conductivity measurement; 4) filtration and retention of insoluble particles for microscopy; 5) dilution or vacuum-driven concentration of samples to accommodate instrument working ranges; 6) removal of gas bubbles from sample aliquots; 7) unidirectional flow (check valves); 8) active flow-path selection (solenoid-actuated valves); 9) metered pumping in 100 nL volume increments. The SPLIce manifold, made of three thermally fused layers of precision-machined cyclo-olefin polymer, supports all fluidic components (Figure 1) and integrated microchannels (125 x 250 m). Fluid is pumped by a stepper-motor-driven pump (Lee Co.). The functionality of the integrated MEMS pressure sensor (Honeywell) and passive check valves (Figure 2) were tested in conjunction with our newly designed integral bubble traps (Figure 3) and hydrophobic membrane-based concentrator (Figure 4). The concentrator (initially tested as a standalone component) demonstrated 5-fold vacuum-evaporative concentration. Polyethylene fused bead beds (PEFBBs; 50 porosity) store drylyophilized buffers, calibrants, and fluorescent dyes, and also promote mixing of sample with calibrant, dye, or H2O. Software-controlled automated tests demonstrated successful 1) fluid delivery to each component 2) valve and pump synchronization 3) sample aliquot delivery to instrument interface ports, and 4) rehydration of vacuum-dried fluorescent dye. In Figure 5, fluorescein on PEFBBs was rehydrated for 15 min using a pump-delivered water aliquot; it is displaced as H2O enters the bottom of the channel and pushes the dye into a check valve. Ultimately, SPLIce will fluorescently label amino acids in the sample for microchip-based electrophoretic (MCE) chiral separation and detection to seek and quantify key organic bio-signatures [5]; it will also deliver sample to a microfluidic version of WCL (mWCL) to measure soluble ions and redox-active species.

Life detection↗

Path Sampling for Rare Events Boosted by Machine Learning

The study by Jung et al. introduced Artificial Intelligence for Molecular Mechanism Discovery (AIMMD), a novel sampling algorithm that integrates machine learning to enhance the efficiency of transition path sampling (TPS). By enabling on-the-fly estimation of the committor probability and simultaneously deriving a human-interpretable reaction coordinate, AIMMD offers a robust framework for elucidating the mechanistic pathways of complex molecular processes. Here, this commentary provides a discussion and critical analysis of the core AIMMD framework, explores its recent extensions, and offers an assessment of the method’s potential impact and limitations.

Minh, Porhouy [Univ. of Minnesota, Minneapolis, MN↗

Potential Mars Surveyor 2001 Landing Sites: Low-Elevation Cratered "Highlands" in Central and Eastern Sinus Meridiani and Near Amenthes Fossae

The main scientific goal for the Mars Surveyor Program 2001 (MSP 01) landed mission is to collect and characterize 91 rock and 13 soil core samples using an integrated instrument suite onboard the Athena Rover. If possible, these samples will be retrieved and returned to Earth via a MSP 05 or MSP 07 mission. Preliminary engineering constraints for the MSP 01 landing site call for a location that lies between 15 S and 30 N, and below about 2 km elevation (based on Viking-era topography). Desirable landing sites for MSP 01 are to be located "in the ancient highlands where the environmental conditions may have been favorable to the preservation of evidence of possible prebiotic or biotic processes including the emergence (and, potentially, the persistence) of life". We interpret this to mean that the desirable sites include those that have evidence of aqueous sediments that might have been deposited during the Noachian and/or Hesperian Epochs of Mars' history. In addition to the search for subaqueous sedimentary deposits, we took into consideration the fact that the rover, Athena, will need to be able to access these materials. Thus, a site where aeolian deflation has occurred might be desirable because it might expose, in situ, layered sedimentary deposits. Deflated areas, of course, might include potential landing hazards in the form of meterscale buttes and mesas (e.g., Christmas Lake Valley, OR), thus careful study of such sites with high resolution images will be required before a decision is made to land. We have been examining three regions that have potential to be considered for MSP 01 landing sites. This work is based on Viking (VIS, IRTM) and Phobos 2 (Termoskan) observations and should be regarded as preliminary because we believe that the final site selection should also be based upon analysis of Mars Global Surveyor observations that help constrain mineralogy (TES) and local geomorphology (MOC, MOLA). (1) Eastern Sinus Meridiani Region (proposed by K. S. Edgett) Sinus Meridiani is a persistent low-albedo (< 0. 16) region on the martian equator that has been recognized for about 400 years. All of Sinus Meridiani is below the 2 km elevation constraint for MSP 01. The region includes cratered highlands, valley networks, aeolian dunes, and possible aqueous sedimentary deposits. The landing site study region is located in the eastern portion of Sinus Meridiani. It is bounded by latitudes 10 S to 2 N, longitudes 355 W to 345 W, and the elevations are mostly 1-2 km. The center of this area contains a medium-albedo (0.19-0.21), relatively smooth-surfaced deposit that was suggested by Rice to be a lacustrine deposit. Several potential landing areas can be suggested within this region. Based on Viking and Phobos 2 data, the favored sites so far are centered at 7.6 S, 346.9 W and 0.8 S, 349 W. Thermal inertias are 3.2-7.0 x 10(exp -3) cal /sq cm s(exp -0.5)/K; and rock abundances are around 2-6%. The site at 7.6 S, 346.9 W is at the southern end of the smooth, medium-albedo unit that might have a lacustrine origin. At this location, numerous channels appear to have drained toward the smooth unit. Viking images from orbit 747A show this area at about 15 m/pixel ground resolution. The images reveal that aeolian deflation has occurred along the deposit's margins. Bright (i.e., albedo >= 0.21) aeolian dunes are present on the channel floors and in some of the depressions on the smooth unit. The bright, apparently active dunes might consist of material (perhaps lakedeposited sands) that has been eroded from the smooth unit. The site at approximately 0.8 S, 349 W is selected because it offers an opportunity to solve a long-standing puzzle about Mars remote sensing. There are three main "color" units on Mars: "dark red, dark gray, and bright red". This landing site would allow the Athena rover an opportunity to investigate all three materials within close proximity (the best place on Mars to do so). There are no high resolution (better than 100 m/pixel) Viking or Mariner images of this site. (2) Central Sinus Meridiani Region (proposed by K. S. Edgett and T. J. Parker) Central Sinus Meridiani is characterized by two types of surfaces [4]. One is like typical martian cratered highlands elsewhere- there are old valley networks and old impact craters. The other is relatively smooth and flat. These two units are in contact around 3.1 S between 5 W and 4 E longitudes. Valley networks- including one at 6'S, 358 W that rivals the Grand Canyon of Arizona- once drained toward the smooth unit. Edgett and Parker [4] proposed that the smooth unit might consist of sediments laid down in a large Noachian-aged sea/ocean that would have covered much of the northern hemisphere. Schultz and Lutz [I I I suggested that it is a paleopolar layered deposit. Regardless, the smooth unit where it contacts the cratered terrain would make an excellent site for Athena rover to investigate. The site is best seen in Viking high resolution images from orbits 408B (about 30 m/pixel) and 746A (about 12 m/pixel). These images suggest that aeolian deflation has occurred along the margin of the smooth unit, and this deflation has exposed horizontal larrs of material. The elevation is about 0.5 km; thermal inertias are 6.5-8.0 x 10(exp -3) cal /sq cm s(exp -0.5) / K; rock abundances are 2-4%; and the surface is probably sandy with dark drifts and ripples but almost no actual dunes. We suggest a landing around 3.2 S, 3.0 W would test the aqueous sediment hypothesis and provide a potentially smooth surface on which to land. (3) Amenthes Fossae Region (proposed by S. N. Huntwork and K. S. Edgett) The Amenthes Fossae are a series of graben/fissures that are circumferential to the southeast side of Isidis Planitia. These fissures cross a variety of ancient, heavily cratered Noachian terrain and younger, Hesperian and Amazonian terrain. We focused our search on a region 0-15 N, 250 - 270 W. Elevations are -0.5 to 2 km. Depending upon whether Isidis Planitia was ever a water-rich environment, this region might have been influenced by aqueous sedimentation. Valley networks are common, and they drained toward the north and northwest. We focused our work on a set of Viking orbiter high-resolution images, 719A 1-48. These have resolutions 16-24 rri/pixel. We examined images 20-23, centered at 2 N, 258 W. This site, on the plains just southwest of a 42 km-diameter crater, includes a valley network channel, a relatively young crater ejecta deposit, a few buttes composed of presumably ancient, Noachian bedrock, and a "plains" unit. The plains might make an ideal landing surface, except for the presence of some fine-scale ridges (oriented approximately N-S). The ridges are probably yardangs, thus this site offers a place where aeolian deflation has probably exposed some of the layered rock units that comprise the "plains". Thermal inertias are 7.9-8.3 x 10(exp -3) cal/sq cm s(exp -0.5) /K and rock abundances are 10-15%. A rover traverse might include the opportunity to go down to the floor (and sample along the walls) of the valley network channel at 2 N 258.1 W.

Edgett, K. S.↗

Mars Sample Receiving Facility Research and Development to Enable Preservation, Safe Containment, and Scientific Research of Martian Samples on Earth

NASA and ESA are working together to plan a joint campaign to potentially bring back the first Martian samples to Earth in the early 2030s. On the surface of Mars, the Mars 2020Perseverance Rover is selecting and packaging samples that could be returned to Earth for careful examination by an international team of scientists. In preparation for this historic sample return, advance planning is underway to design and build a Mars Sample Receiving Facility (SRF) in the mid-2020s. In 2022, a Mars Sample Receiving Facility Assessment Study(MSAS) will be conducted to further define construction modality and capability options for a facility in the conterminous United States. Since Mars Sample Return (MSR) is currently categorized as a planetary protection restricted Earth return, this new facility would feature biosafety level 4 (BSL-4)-like high containment to protect Earth’s biosphere from any potential hazard. In addition, the facility also requires integration of cleanroom technologies to mitigate against terrestrial contamination and preserve sample integrity for science investigations. The integration of both clean handling and high containment requires significant technology research and development (R&D) by the mid-2020s to support the definition and planning of a SRF before commencing the site specific design phase. The SRF project will need to solidify the inorganic, organic, and biological contamination control (CC) requirements for the facility. This could entail a translation of Mars 2020 mission CC requirements for geologic material to engineering requirements for surfaces and airborne molecular contamination inside isolators and cleanrooms. In tandem, the project will need to determine precision cleaning and sterilization approaches for cleanrooms, isolators, equipment, and tools. Initial material selections for the facility construction materials, cleanrooms, isolators, and BSL-4 suits/garments are an important activity. The recent construction of the OSIRIS-REx and Hayabusa2 curation cleanroom laboratories greatly benefited from early materials testing, before the design phase, to reduced organic outgassing and particulate shedding inside the laboratory. While the early biohazard investigations in the SRF may deem the samples safe to release to laboratories throughout the world, sterilization methods need to be defined to safely release Martian samples. One key aspect of enabling simultaneous sample containment and cleanliness is the concept of a Double-Walled Isolator (DWI) that ESA has been pursuing. Further R&D is needed about DWIs, sample handling, and instrumentation interfaces before beginning the SRF site specific design phase. A working isolator/DWI engineering model should be developed and fabricated. Isolator sizes, connections, pass-through antechambers, and configurations and basic interfaces with instruments and tools as well as the use of robotic, mechanical, and/or human manipulation need to be considered. Inert high purity gas supply (one-pass or recirculation) and other isolator utilities must be determined. Special accommodations for large instruments (e.g., XCT,SEM, etc.) need to be developed. Techniques for opening the sample tubes packaged by M2020and extracting the headspace gas while keeping samples pristine will be challenging, requiring additional R&D, and engagement of the M2020 project. In addition, careful micromanipulation for subdivision and packaging of samples will also need to be included. These combined R&D activities are important before commencing the SRF design phase to ensure safe biohazard containment, sample preservation, and science integrity for the samples that would be studied in the SRF and in laboratories around the world.

mars sample return↗

Versatile soil gas concentration and isotope monitoring: optimization and integration of novel soil gas probes with online trace gas detection

Abstract. Gas concentrations and isotopic signatures can unveil microbial metabolisms and their responses to environmental changes in soil. Currently, few methods measure in situ soil trace gases such as the products of nitrogen and carbon cycling or volatile organic compounds (VOCs) that constrain microbial biochemical processes like nitrification, methanogenesis, respiration, and microbial communication. Versatile trace gas sampling systems that integrate soil probes with sensitive trace gas analyzers could fill this gap with in situ soil gas measurements that resolve spatial (centimeters) and temporal (minutes) patterns. We developed a system that integrates new porous and hydrophobic sintered polytetrafluoroethylene (sPTFE) diffusive soil gas probes that non-disruptively collect soil gas samples with a transfer system to direct gas from multiple probes to one or more central gas analyzer(s) such as laser and mass spectrometers. Here, we demonstrate the feasibility and versatility of this automated multiprobe system for soil gas measurements of isotopic ratios of nitrous oxide (δ18O, δ15N, and the 15N site preference of N2O), methane, carbon dioxide (δ13C), and VOCs. First, we used an inert silica matrix to challenge probe measurements under controlled gas conditions. By changing and controlling system flow parameters, including the probe flow rate, we optimized recovery of representative soil gas samples while reducing sampling artifacts on subsurface concentrations. Second, we used this system to provide a real-time window into the impact of environmental manipulation of irrigation and soil redox conditions on in situ N2O and VOC concentrations. Moreover, to reveal the dynamics in the stable isotope ratios of N2O (i.e., 14N14N16O, 14N15N16O, 15N14N16O, and 14N14N18O), we developed a new high-precision laser spectrometer with a reduced sample volume demand. Our integrated system – a tunable infrared laser direct absorption spectrometry (TILDAS) in parallel with Vocus proton transfer reaction mass spectrometry (PTR-MS), in line with sPTFE soil gas probes – successfully quantified isotopic signatures for N2O, CO2, and VOCs in real time as responses to changes in the dry–wetting cycle and redox conditions. Broadening the collection of trace gases that can be monitored in the subsurface is critical for monitoring biogeochemical cycles, ecosystem health, and management practices at scales relevant to the soil system.

54 ENVIRONMENTAL SCIENCES↗

Method and apparatus for frequency spectrum analysis

A method for frequency spectrum analysis of an unknown signal in real-time is discussed. The method is based upon integration of 1-bit samples of signal voltage amplitude corresponding to sine or cosine phases of a controlled center frequency clock which is changed after each integration interval to sweep the frequency range of interest in steps. Integration of samples during each interval is carried out over a number of cycles of the center frequency clock spanning a number of cycles of an input signal to be analyzed. The invention may be used to detect the frequency of at least two signals simultaneously. By using a reference signal of known frequency and voltage amplitude (added to the two signals for parallel processing in the same way, but in a different channel with a sampling at the known frequency and phases of the reference signal), the absolute voltage amplitude of the other two signals may be determined by squaring the sine and cosine integrals of each channel and summing the squares to obtain relative power measurements in all three channels and, from the known voltage amplitude of the reference signal, obtaining an absolute voltage measurement for the other two signals by multiplying the known voltage of the reference signal with the ratio of the relative power of each of the other two signals to the relative power of the reference signal.

Cole, Steven W.↗

Investigation of Ion-Irradiated Beryllium Carbide (Be 2 C) for High-Temperature Nuclear Reactor Moderators

Beryllium carbide (Be 2 C) is an attractive alternative to graphite as a moderator material because of its high melting point, moderating efficiency, and theoretical environmental compatibility in MSRs, FHRs and HTGRs. However, its behavior under neutron irradiation is not yet known. Research on otherwise promising beryllium compounds are restricted because of the toxic nature of the material. For this work, a novel experiment was designed to safely irradiate beryllium-containing samples at The Michigan Ion Beam Laboratory (MIBL). Using this new capability, Be 2 C samples were irradiated with 9 MeV C 3+ ions from 2 dpa to 30 dpa, at temperatures up to 500 °C. Samples were characterized to investigate radiation tolerance. No evidence of phase precipitation, dislocation loops, or amorphization was observed up to 30 dpa, suggesting good radiation tolerance. One sample left in air for ~3 months oxidized slowly and lost structural integrity, while a sample kept in argon did not, suggesting that Be 2 C is not suitable for service in moist environments, but maintains its integrity in dry environments.

22 - GENERAL STUDIES OF NUCLEAR REACTORS↗

Mars Sample Thermal Control During Mars Ascent and Orbit

Although NASA has no official plans at this time for a mission to return samples from Mars, the Program Formulation Office of the Mars Exploration Program sponsors ongoing mission concept studies, systems analyses, and technology investments which explore different strategies for the potential return of samples from Mars, consistent with the charter of the program and stated priorities of the science community. Maintaining the thermal integrity of collected samples would be very important. In general, samples would be collected, sealed inside tubes, and left on the surface for later retrieval. They would then be inserted into an OS (Orbiting Sample), and carried to a Mars or Solar orbit via a MAV (Mars Ascent Vehicle). Subsequently, an Earth return vehicle would rendezvous with the OS and bring it back to Earth. During ascent from Mars, the OS could serve as the nose cone of the MAV and would be subjected to significant aerodynamic heating from the Martian atmosphere. Once the OS is released from the MAV, its external surface would be exposed to potentially several years of sunlight, eclipse, planetary IR, albedo, and space. The challenge is to ensure that these samples are kept at thermally moderate conditions to preserve their integrity in these widely different environments. Various thermal techniques have been investigated to achieve sample thermal control: use of thermal protection shields and surfaces (ablative and non-ablative) to protect them from adverse exposure to ascent heating, as well combinations of thermo-optical coatings during the orbital phase. The work described herein is part of this ongoing effort & will describe the key challenges related to the thermal control of the potential Mars samples during these phases and the corresponding schemes to overcome them.

Bhandari, Pradeep↗

Reducing Organic Contamination in NASA JSC Astromaterial Curation Facility

Future robotic and human spaceflight missions to the Moon, Mars, asteroids and comets will require handling and storing astromaterial samples with minimal inorganic and organic contamination to preserve the scientific integrity of each sample. Much was learned from the rigorous attempts to minimize and monitor organic contamination during Apollo, but it was not adequate for current analytical requirements; thus [1]. OSIRIS-REx, Hayabusa-2, and future Mars sample return will require better protocols for reducing organic contamination. Future isolation con-tainment systems for astromaterials, possibly nitrogen enriched gloveboxes, must be able to reduce organic and inorganic cross-contamination. In 2012, a baseline study established the current state of organic cleanliness in gloveboxes used by NASA JSC astromaterials curation labs that could be used as a benchmark for future mission designs [2, 3]. After standard ultra-pure water (UPW) cleaning, the majority of organic contaminates found were hydrocarbons, plasticizers, silicones, and solvents. Hydro-carbons loads (> C7) ranged from 1.9 to 11.8 ng/cm2 for TD-GC-MS wafer exposure analyses and 5.0 to 19.5 ng/L for TD-GC-MS adsorbent tube exposure. Plasticizers included < 0.6 ng/cm2 of DBP, DEP, TXIB, and DIBP. Silicones included < 0.5 ng/cm2 of cyclo(Me2SiO)x (x = 6, 8, 9, 10) and siloxane. Solvents included < 1.0 ng/cm2 of 2-cyclohexen-1-one, 3,5,5-trimethyl- (Isopho-rone), N-formylpiperidine, and 2-(2-butoxyethoxy) ethanol. In addition, DBF, rubber/polymer additive was found at < 0.2 ng/cm2 and caprolactam, nylon-6 at < 0.6 ng/cm2. Reducing Organics: The Apollo program was the last sam-ple return mission to place high-level organic requirements and biological containment protocols on a curation facility. The high vacuum complex F-201 glovebox in the Lunar Receiving Labora-tory used ethyl alcohol (190 proof), 3:1 benzene/methanol (nano grade solution), and heat sterilization at 130degC for 48 hours to reduce organic contamination. In addition, both heat sterilization and peracetic acid sterilization were used in the atmospheric de-contamination (R) cabinets. Later, Lunar curation gloveboxes were degreased with a pressurized Freon 113 wash. Today, UPW has replaced Freon as the standard cleaning procedure, but does not have the degreasing solvency power of Freon. Future Cleaning Studies: Cleaning experiments are cur-rently being orchestrated to study how to degrease and reduce organics in a JSC curation glovebox lower than the established baseline. Several new chemicals in the industry have replaced traditional degreasing solvents such as Freon and others that are now federally restricted. However, these new suites of chemicals remain untested for lowering organics in curation gloveboxes. 3M's HFE-7100DL and DuPont's Vertrel XF are currently being tested as a replacement for Freon 113 as a degreaser at JSC cura-tion facilities. In addition, the use of UPW as a final rinse is be-ing tested, which presumably can maintain a lower total organic carbon load than the filtered purity of chemical solutions. References: [1] Allton J.H. et al. (2012) LPS XLIII, 2439; [2] Calaway M.

Calaway, M. J.↗

Organic Contamination Baseline Study in NASA Johnson Space Center Astromaterials Curation Laboratories

Future robotic and human spaceflight missions to the Moon, Mars, asteroids, and comets will require curating astromaterial samples with minimal inorganic and organic contamination to preserve the scientific integrity of each sample. 21st century sample return missions will focus on strict protocols for reducing organic contamination that have not been seen since the Apollo manned lunar landing program. To properly curate these materials, the Astromaterials Acquisition and Curation Office under the Astromaterial Research and Exploration Science Directorate at NASA Johnson Space Center houses and protects all extraterrestrial materials brought back to Earth that are controlled by the United States government. During fiscal year 2012, we conducted a year-long project to compile historical documentation and laboratory tests involving organic investigations at these facilities. In addition, we developed a plan to determine the current state of organic cleanliness in curation laboratories housing astromaterials. This was accomplished by focusing on current procedures and protocols for cleaning, sample handling, and storage. While the intention of this report is to give a comprehensive overview of the current state of organic cleanliness in JSC curation laboratories, it also provides a baseline for determining whether our cleaning procedures and sample handling protocols need to be adapted and/or augmented to meet the new requirements for future human spaceflight and robotic sample return missions.

Calaway, Michael J.↗